Method of molding articles.



UNITED srA'rEs LEO n. BAEKELAND, or xonxnns, NEW Yoax.

mnrnon or MOLDING ARTICLES.

No Drawing.

To all whom it may concern:

Be it known that I, LEO H. BAEKELAND, a citizen of the United States, residing at Yonkers, in the county of Westchester and State of New York, have invented certain new and useful Improvements in Methods of Moldin Articles, of which the following is a'ipeci cation...

n my rior U. S. applications, Ser. Nos. 383,684, led July 13, 1907,'397,560, filed October 15, 1907, and 405,021, filed December 4, 1907, I have described several methods f obtaining infusible and insoluble conupon each other and yield a product consisting of two liquids which will separate or stratify on standing. The supernatant liquid is an aqueous solution which contains the water resulting from the reaction or added with the reagents, whereas the heavier liquid is oily or viscous in character and contains the initial products of chemical condensation. The liquids are readily 'separated, andthe aqueous solution may be re-- jected, or the water may be eliminated'by evaporation. The oily or viscous li uid obtained as above described is foun to be soluble in or miscible with alcohol, acetone, phenol, and other solvents, but is only partially and imperfectly soluble in benzol. This product may assume a pasty or semisolid state when cooled, or may even assume a solid or brittle state, but is again liquefied when heated, and this alternate solidification and liquefaction may be repeated so lopg as the product'does not become transformed into the intermediate or into the final eondensation products hereinafter described. This product will be hereinafter referred to as the initial condensation product.

If the initial condensation; product be heated in an open vessel at temperatures above 100 G., the mass will foam, emit Specification of Letters Patent.

Patented Nov. 16, 1909.

Application filed January 28, 1909. Serial No. 474,869.

vapors,-and yield a hard irregular and porous body, infusible by further heating and insoluble in alcohol, acetone and pheno In order to avoid the production of a porous mass it has been proposed to harden the mitial condensation product at temperatures below 100, but suc 1 hardening is extremely slow and applicable only to relatively thin layers of .material. In closed ,vessels or molds in which ressure may be usedto counteract the tendency of the mass to liberate gases or vapors, as described in my application above referred to, the hardening may be accomplished much more qluickl an is more .complete, the final ro uct eing homogeneous or free from ,al porosity, insoluble in alcohol, acetone, benzol, phenol or glycerin, or any other known solvent, and less elastic than hard rubber but much heat, infusible at all tem eratures. The roduct thus obtained is hereinafter referred o as the final. condensation product.

Under proper conditions there -may be produced a condensation product which is intermediate in character between the initial and final products abovedescribed, and which is hereinafter referred to as the intermediate condensation product. This intermediate product is solid at all temperatures, more or less hard when cold, but elastic when slightly heated, and is capable at normal or higher temperatures of yielding to pressure but will resume its original shape if pressure be discontinued; further a plication of heat will soften it to a cona liquid/ The product is insoluble in alcohol, glycerin, formalin, or a mixture of the two'latter compound" but swells in phenol and in acetone without complete solution. For convenience I will hereinafter refer to both the initial and intermediatecondensation products as par.tial reaction products, in contradistinc'tionto the insoluble and indensation product.

For the purposes of the present invention I first obtain either of the partial reaction products, that is'to say the initial condensafusibl' mass which constitutes the final conharder and considerably more resistant to V siderable extent but will not convert it into tion product or the intermediate condensation product in solid form; this result is readily attained by a sufliciently prolonged i heating or by adding the proper proportion of a suitable condensing agent, preferably a base as described in my prior-application -Ser.No.397,5.60. When this ointisreached considerably higher temperatures, approach:

ing orexceeding 200 0., give improved results. The use of these high tem eratures allows the rapid and complete ormation of-the final condensation product, which is insoluble and infusible and does not soften or softens only Very slightly under application of heat. Or a lower temperature or shorter time of molding may be used, the molded objects being then taken from the mold and transferred to a' vessel where they can be heated further under suitable pressure, this rocedure having theadvantage of a less pro onged use of the mold.

Instead of using theimaterial alone it is often desirable to incorporate with it so called; fillers, as for example inorganic or organic fibrous or cellular materials such as asbestos or wood pulp or other suitable'substances which may impart a special color or special properties to the product, or which may cheapen the cost of production or facilitate the act of molding.

The fillers'or additional incorporated substances may be added directly to the phenol or the formaldehyde or to any partial reaction product derived from them, and. the chemical reaction carried on to such point that the mass has become sufliciently solid to permit subdivision by pulverizing or grinding, care being taken to avoid carrying the reaction to the point where the henol and formaldehyde are transformed into the final insoluble and infusible condensation product.

The addition of suitable condensing agents, and especially the addition of bases as described 111' my prior application Ser. No. 397 ,560, enables me to reach the desired stage of the reaction quickly and surely. After the mass has reached the proper stage it is'ground or pulverized, after which it is molded in the hydraulic press as above described.

Molded articles produced by any of the methods above described may be afterward coated by dipping or varnishing with a thin layer of condensation'product, which is later transformed-into the final condensation product by any of the methods described in my prior applications. This treatment permits the use of compounds containing much filling material and which on this account would otherwise be undesirably porous; the treatment also imparts a. gloss to the molded articles. The same result in surfacing the articles can be vattained by dusting or coating the walls of the mold with the unmixed powdered partial reaction product or a mixture veryrich in the latter product, or by first'coating the mold in this manner and afterward with the same product mixed with an appropriate amount of filler, then pressing and treating as usual. I

I am fully aware that ground mixtures containing resinous materials have been heretofore used in molding objects. In the present case, however, the problem is entirely novel, because the final condensation product which enters into the constitution of the article is incapable of being welded by any known method to a. compact, homogeneous and strong mass. Under the circumstances, it is necessary tobrin the initial or the intermediate product 0 condensation into such a physical state that it can be subdivided and practically employed for rapid and effective mixing and molding; and it is further necessary that durin the act of molding or heating the further 0 emical reaction should occur which transforms the partial reaction product into a final condensation product of maximum toughness, hardness, and physical and chemical inertness. It is necessary to deal not merely with a physical treatment which shapes the compressed body, but with a chemical action which either completes the process of condensation or starts a phenomenon of polymerization which'brings about the desired result. To mold in the hydraulic press any of the viscous, pasty or liquid mlxtures above described involves considerable trouble and expenditure of time, whereas by means of the method herein described I am able to accomplish the moldin in from five to ,ten minutes; or if the ob ects be small and the temperature sufficiently high the molding maybe completed in two minutes or even less, thus securing great industrial advantages.

A By the word phenol as used in the claims I intendto include as equivalents the homologues of phenol; and by the word formaldeh de, I include the polymers of formaldehy e.

I claim:

1. The method of molding articles which consists in comminuting a partial reaction product of phenol and formaldehyde, molding the mass under pressure, and transforming the same into an insoluble and infusible condensation product.

2. The method of molding articles which consists incomminuting a partial reaction product of phenol and formaldehyde, molding the mass under pressure, and transforl'ning the same in the mold into an insoluble and infusible condensation product.

3. The method of molding articles, which consists 1n pre aring a comminuted mixture of a partla reaction product of phenol and formaldehyde and a filling material,

molding said mixture, and transforming the partial reaction product into an insoluble and infusible final condensation product. a 4. The method of molding articles, which consists in preparing a eomminutedmixture of a partial reaction product of phenol and formaldehyde and a filling material, mold-,- ing said mixture, transforming the partial 10 reaction product into an insoluble and infusiblefinalcondensation product, and roviding the molded article with a snr ace layer containing a larger; proportion of said final condensation product.

In testimony whereof, I aifix my signa 15 ture in presence of two witnesses.

. LEO H. BAEKELAND. 'Witnesses H. S. TARBELL, MARY L. SHORT. 

